Nanocrystalline Diamond Coating around Sphere Analysis

Nanocrystalline Diamond Coating around Sphere Analysis Mechanical Properties and Uniformity of Nanocrystalline Diamond coating around Sphere Hongyun Chen Nanocrystalline diamond coatings were deposited on spheres used for ball bearing. The nanocrystalline coatings with a grain size of 50nm were confirmed by the surface morphology and composition analysis. The hardness of the coating is 20-40GPa tested by nanoindentation, which is higher than that of tungsten carbide and silicon nitride substrates. The coating around the sphere observed from the Micro CT images is uniform with a thickness of 12ÃŽ ¼m. keywords: solid lubricating coating, nanocrystalline diamond, mechanical properties Introduction Mechanical parts are often used under extreme environment such as high temperature, large load, radioactive and high vacuum, and so on. A wear-resistant, lubricating coating can protect the mechanical parts and ensure their reliability under these extreme conditions1, 2. The advantages of diamond coating with high hardness, high elastic modulus, outstanding wear resistance, low friction coefficient and good chemical stability make it to be an expected solid lubricating coating3, 4. The protective coating, e.g. diamond like carbon (DLC) coating deposited on metals and some other materials can protect the interface of the metals from crack, but also reduce the frictional wear of the opposing surface due to the excellent tribological properties such as extremely low friction and wear resistance. Costa et al5. deposited (DLC) coating with a thickness of 2ÃŽ ¼m on silicon and carbonitride using pulsed-DC discharge and studied the tribological behavior of DLC coating. Their results showed that the increase in surface roughness reduced the friction coefficient, and wear rate of the carbonitride as the interlayer decreased three orders compared to that of silicon. Xie et al6. grew DLC coating with 600nm thickness on silicon wafer using microwave plasma chemical vapor deposition (MPCVD). It seemed that surface roughness, adhesion and debris accumulation collectively affected the frictional behavior while the tribological behavior of DLC coating mainly depended on the co ating and its adhesion to the substrate. Gruen et al7. successfully deposited the nanocrystalline diamond coating with average grain size of 5-13nm on silicon at 750à ¢Ã¢â‚¬Å¾Ã†â€™ by MPCVD. After that, there were much investigation of the nanocrystalline diamond coating, but the nanocrystalline diamond coating grown on the spheres are very few. B Lunn et al8. from Hull University deposited micro diamond coating with thickness of 3ÃŽ ¼m on a sintered carbide (6%Co) ball of 15mm in diameter with a special support system in a hot filament chemical vapor deposition (HFCVD) chamber. The present work focused on that nanocrystalline diamond coatings were deposited on the sintered carbide spheres and silicon nitride spheres used for ball bearing to improve the wear-resistance. The mechanical properties and uniformity of the coating were evaluated by Micro CT and nano indenter. Experimental By rotating the substrate holder, uniform diamond coatings around spherical substrates with 1-3mm diameter were deposited by a lab-made MPCVD reactor. Tungsten carbide (WC-6 wt.% Co) spheres and silicon nitride spheres were pitched up as the substrates. The cobalt as the adhesive of tungsten carbide would convert the diamond into graphite, resulting in decrease in adhesion between coating and substrate. So firstly diluted nitric acid was used for processing the tungsten carbide spheres in order to selectively remove the cobalt of the surface9. Then, the spheres were scratched using 1-10ÃŽ ¼m diamond powders by ultrasonic method, and rinsed in alcohol and dried prior to deposition. The nanocrystalline diamond coating was deposited for 20-60h at following parameters: total gas pressure was 4KPa, microwave power was 1400W, the substrate temperature was 870à ¢Ã¢â‚¬Å¾Ã†â€™, 2.2% methane diluted in hydrogen. The Raman spectroscopy (LabRAM HR, HORIBA Jobin Yvon S.A.S, France) with a laser as light sources (wavelength 532nm) was used to analyze the quality of diamond coating on different substrates. The surface morphology was investigated by scanning electron microscopy (SEM, JSM-7500F, Hitachi, Japan) to measure the crystalline grain size. An atomic force microscopy (AFM, MFP-3D, Asylum Research, USA) was applied for quantitative the surface roughness determination on a 20Ãâ€"20ÃŽ ¼m scanned area. The mechanical properties were measured by MTS nano indenter (G200, MTS, USA) at an approach velocity of 5nm/s. The thickness and the uniformity of the diamond coating were investigated by Micro CT (ÃŽ ¼CT100, SCANCO, Switzerland). Results and discussion 3.1. surface morphology The surface morphologies of coatings deposited on different substrates can be seen in Fig.1a and c respectively, and b and d are the high magnification of images. Both the samples were treated under the same conditions. It is evident that there is no big difference between coating deposited on tungsten carbide sphere and silicon nitride sphere. The obtained coatings on both substrates have cauliflower structure with a grain size of about 50 nm. The surface roughness is very important for solid lubricating application where a smooth coating surface can decrease the frictional wear. Table 1 shows the change in roughness due to the thickness change of coating on tungsten carbide using AFM method. The roughness of the coating followed the trend in thickness, which was increasing with the rise of the thickness of coating. The roughness of the coating with 5ÃŽ ¼m thickness was under 150nm. Both RMS roughness and the average (Ra) roughness were between 100nm and 210nm lower than the peak-valley (P-V) roughness. The latter had higher roughness values in the order of one micron, which accounted for the cauliflower structure on the surface of the coating as shown in Fig.1. The rough surface does harm to the solid lubricating application. So the roughness will be decreased through post treatment e.g. chemical mechanical polishing. 3.2. Uniformity and thickness The small sphere makes it hard to measure the thickness and the uniformity of the diamond coating. SEM image of the cross section is usually used to show the thickness and uniformity of the coating. However, only one intersecting surface is observed, which can’t represent the whole sphere. Micron CT can get a 3D image of the coating and directly give the whole feature of the coating. Because the metal absorbs the X-ray, the coating on silicon nitride which is inorganic material was measured. Fig.2 is the CT image of the diamond coating around sphere. Fig.2a and b are the 2D and 3D images of the sphere and c is the 3D CT image of the shell whose silicon nitride substrate is removed through analysis software simulation. As the images shown, the coating is uniform and no obvious protuberance on the surface can be observed. The cross section of coating in Fig.4a indicated that the concentricity between substrate and coating was maintained to assure uniform coating thickness. No separation between the silicon nitride substrate and coating was observed, suggesting that the diamond coating attached the sphere tightly. Fig.3 shows the thickness distribution of the coating. The thickness of coating is between 10 to 14ÃŽ ¼m among which 12ÃŽ ¼m is dominant. 3.3. Composition CVD diamond coatings with different thickness were characterized by Raman spectroscopy as shown in Fig.4, a and b were the coating with 5ÃŽ ¼m thickness, and c and d were the coating with 12ÃŽ ¼m thickness. The peak at 1332cm-1 is the characteristic of the diamond lattice which can be used to identify diamond. Two sharp peaks at 1337.87cm-1 and 1333.64cm-1 in Fig.4a and b proved that the composition of coating was in relation to diamond. Both of the two peaks have frequency shift caused by the compressive stress10. This accounted for the mismatch of the thermal expansion coefficient between diamond and substrate. Especially, the value of the tungsten carbide(4.36Ãâ€"10−6/ °C, 20 °C) is larger than 1.18Ãâ€"10-6/ °C (20 °C) of diamondà ¯Ã‚ ¼Ã…’resulting in the far more upshift of the tungsten carbide shown in Fig.4a. The value of silicon nitride (2.8Ãâ€"10−6/ °C, 20 °C), which is close to that of diamond, produced less residual compressive stress. With the thickness of coating increasing, there was almost same frequency shift shown in Fig.4c and d. Compared with Fig.4a and b, the diamond peak of the thicker coating has a large upward shift that attributed to the increase in compressive stress with thickness increasing. The compressive stress is also related to other factors such as defects, composition of coating. The stress from defects and composition appeared to be dominant in thick coating. The features at 1145cm-1 and 1490cm-1 are possibly related to acetylene C–H chains proposed by R. Pfeiffer11 and his colleague. Their study considered this acetylene C–H chains existed in the boundaries of nanocrystal diamond. Those bands around 1140cm−1 and 1490cm−1 were usually observed in nanocrystalline diamond coating. So Fig.4a and b confirmed the deposited coatings were nanocrystalline diamond, which is consistent with the result of the SEM. In addition, the coating got flexibility to fit curved surface of sphere because of the acetylene C–H chains in coating. In Fig.4c and d, the peaks at 1580cm-1 is labeled as G peaks which are due to the sp2 sites. Compared with Fig.4a and b, the G peak of the graphite is obviously observed on Fig.4c and d. Although G peak at 1560cm-1 possibly overlapped the peak at 1490cm-1, it was obvious that the composition of the thicker coating was different from that of the thinner coating which affected by substrate to some extent. The band at 1146cm-1 is related to nanocrystalline diamond as discussed above. 3.4. Mechanical properties The modulus and the hardness of diamond coatings were characterized by the nano indenter designed by the MTS Company. The sphere was too small to find an applicable flat surface to get an accurate result. The diamond coating deposited on silicon wafer was prepared with the same conditions as the control. As known to all, the hardness and the modulus of the diamond coating prepared by CVD are normally lower than that of the natural diamond. The Fig.5a and c show the modulus and the hardness of the diamond coating deposited on sphere, while the Fig.5b and d exhibit the modulus and the hardness of the diamond coating on silicon wafer deposited in same conditions. The hardness of the coating on sphere was about 20GPa, only a half of that on silicon wafer, and the modulus was only one third of that on silicon wafer. The curved surface and cauliflower structure of the coating on sphere led to lower hardness and modulus measured. The true hardness and modulus of the coating should be higher than that of the measured. In terms of the measured value on silicon wafer, the hardness of coating on sphere was estimated to be 20-40GPa and the modulus was 200-600GPa. Therefore, the diamond coating was expected to improve the wear-resistance of tungsten carbide and silicon nitride substrates whose ha rdness are about 17GPa and 15.6-9.8GPa respectively11, 12. The modulus of coating also increased in comparison with that of silicon nitride substrate. It suggests that the mechanical properties of both the tungsten carbide and silicon nitride are improved for its ball bearing application. Conclusion For the purpose of protecting the spheres used for ball bearing, the diamond coatings were successfully deposited on the spheres. The coating is about 5-12ÃŽ ¼m in thickness depending on the deposition time and is uniform as the result of the Micro CT shown. The surface of coating is not smooth enough due to its cauliflower structure and needs further polish. The hardness tested by the nano indenter was 20-40GPa larger than that of tungsten carbide and silicon nitride. The Raman spectra reveal that the coating deposited on sphere is composed of diamond, acetylene C–H chains and graphite, which are responsible for the improvement of mechanical properties and fitness around sphere.

Ionic

Define and describe ionic and covalent bonds. An ionic bond is a type of chemical bond formed through an electrostatic attraction between two oppositely charged ions. A covalent bond is the chemical bond that involves the sharing of pairs of electrons between atoms. A compound is made when two or more atoms form a chemical bond, linking them together. The two types of bonds are ionic bonds and covalent bonds. In an ionic bond, the atoms are bound together by the attraction between oppositely charged ions. If the electron is shared equally between the atoms forming a covalent bond, then the bond is said to be nonpolar.An electron is more attracted to one atom than to another which forming a polar covalent bond. Ionic bonds are formed between a cation and an anion. Pure ionic bonding cannot exist: all ionic compounds have some degree of covalent bonding. An ionic bond is considered a bond where the ionic character is greater than the covalent character. The larger the difference in ele ctronegativity between the two atoms involved in the bond, the more ionic the bond is. Bonds with partially ionic and partially covalent character are called polar covalent bonds. Ionic bonding is a form of no covalent bonding.Ionic compounds conduct electricity when molten or in solution, but not as a solid. They generally have a high melting point and tend to be soluble in water. The stable balance of attractive and repulsive forces between atoms when they share electrons is known as covalent bonding. For many molecules, the sharing of electrons allows each atom to attain the equivalent of a full outer shell, corresponding to a stable electronic configuration. Covalent bonding includes many kinds of interaction, including ? -bonding, ? -bonding, metal-to-metal bonding, agnostic interactions, and three-center two-electron bonds.The term covalent bond dates from 1939. The prefix co- means jointly, associated in action, partnered to a lesser degree in essence, means that the atoms sh are valence. Molecule H2, the hydrogen atoms share the two electrons via covalent bonding. Covalency is greatest between atoms of similar electronegativity. Covalent bonding does not necessarily require the two atoms be of the same elements, only that they are of comparable electronegativity. Although covalent bonding entails sharing of electrons, it is not necessarily delocalized.

PRACTICAL REPORT ON THE ISOLATION AND IDENTIFICATION OF CODEINE AND PARACETAMOL Essay

Codeine or methyl morphine, an alkaloid, was first isolated in 1832 from raw opium. It concentration ranges from 0.2% to 0.8%. Mostly used for its analgesic, anti-tussive and anti-diarrheal capabilities (Tremlett, Anderson and Wolf, 2010). Paracetamol also known as acetaminophen (n-acetyl-p-aminophenol, APAP) on the other hand, is a useful non- steroidal anti- inflammatory drug (NSAID). It is commonly used in the management of pain and fever in a variety of patients (Kamberi, et al., 2004). Fig 1: Codeine[NCBI, 2009] Fig 2: Acetaminophen[NCBI, 2009] One of the technique involved in the extraction of codeine and paracetamol from its matrix, is the solvent extraction otherwise known as liquid – liquid extraction. This process entails the use of two immiscible liquids usually chloroform and water; in dissolving the sample for two distinctive layers to form after the mixture had been thoroughly shaken together (Rubinson and Rubinson, 1998). Separating the components of the extract, is done through the use of Thin Layer Chromatography. It is one of the standard procedures used in many forensic laboratory when analysizing unknown drugs or mixtures (Howlett and Steiner, 2011). Separation of the mixtures occur based on the pH, polarity of its components, solvent and the thin layer stationary phase (Howlett and Steiner, 2011). METHODS: The finely divided sample was dissolved in 20ml of distilled water. This was then basified with NaOH solution to pH 12 using litmus paper. The resulting solution was later filtered. 1.0ml of chloroform was pipetted into the filtrate. After shaken and combined, two distinctive layers was observed. The bottom layer was extracted thrice using a micro- pipette. On a thin chromatography plate, five spots were placed ( as shown in table 2) and the  plate was developed using chloroform/methanol. This was later visualized with dragendorff’s reagent under the UV light. All separated components were observed, identified and recorded. RESULTS: Table of observed pH SOLUTIONInitial pHFinal pH Basified sample1012 TABLE 1 Table of Retention factor (RF value) Rf = Distance travelled by the substance (cm) Distance travelled by the solvent (cm) SUBSTANCEDistance travelled by substance (cm)Distance travelled by Solvent (cm)Retention factor value (Rf) Chloroform extract3.04.00.75 Codeine positive control3.04.00.75 Paracetamol positive control4.04.01.00 Chloroform (negative control) 3.54.00.86 Diluted sample4.04.01.00 TABLE 2 DIAGRAM: Fig 3: The Developed Chromatographic Plate. DISCUSSION: Running the chloroform extracts and diluted sample together with two positive controls and a negative control on a single chromatographic plate simultaneously, the retention factor(Rf) of five different samples were determined. The RF value of the chloroform extract(0.75) tallied with that of the codeine positive control and that of diluted sample(1.00) with the paracetamol positive control. This tentatively shows that, codeine and paracetamol were present in the sample. The solvent front(i.e distance travelled by the mixed solvents) is 4cm, this is quite close to the distances covered by all separated components(between 3 – 3.5cm), which makes the retention factors, not a true representative of their actual values. It was later discovered that, this is due to not allowing the  chromatographic plate to develop for a longer period of time in the solvent tank. The solvent front also dried up quickly when the plate is taken out., making drawing a line at that point quite diffic ult. Fortunately, this was overcome by the use of visualizing spray and UV lamp. Solvent extraction(liquid-liquid), involved selective movement of components of a substance in microgram to gram quantities between two immiscible liquid phase; its separation and selectivity is based on solubility differences and pH control respectively (Fifield and Kealey, 1995). This was observed when chloroform was added to the basified filtrate. After vigorous shaking and settling down, chloroform being more dense, composed the bottom layer, with the aqueous phase up. Liquid-liquid extraction often involved high volume of organic solvents and poor resolution of mixtures of organic materials (Fifield and Kealey, 1995). Thin Layer Chromatography is usually employed in the qualitative analysis of mixtures of non-volatile compounds like pharmaceuticals (Skoog, et al., 2000). TLC can also be used to confirm the identity of an unknown sample ( Lewis and Evans, 2011). Dissolution of the codeine and paracetamol tablet in distilled water without weighing, shows that, TLC was never designed for semi- quantitative analysis. This is due to difficulties in reproducibly applying aliquots of the mixture to the plate and then recovering all of the separated components from the plate (Skoog, et al., 2000). CONCLUSION: Using the Rf values obtained in the table 2 above and t he visual indicator reaction with the substances under the UV light, codeine was extracted to a high degree during the solvent extraction, tentatively identified by TLC (due to its positive control having the same Rf values with the chloroform extract(0.75) and both were the only one that were seen under the UV light) while paracetamol was extracted to a low degree (due to its positive control having the same Rf with the diluted sample). Multiple compounds can share the same retention factor(Rf) or produce similar chromophores when sprayed with detection reagents (Howlett and Steiner, 2011). The study by Lewis and Evans( 2011) shows that if a spot from an unknown substance is developed on a TLC plate together with a spot from a substance that is suspected to be the unknown, and the two substance are found to have the same Rf value, they are probably the same substance. FUTURE SUGGESTIONS AND RECOMMENDATIONS: Due to the limitation that is associated with using TLC to exactly identify a given sample, minimum standards for drug testing and reporting in the forensic community are recommended by the Scientific Working Group for the Analysis of seized drugs (SWGDRUG) (Howlett and Steiner, 2011). In order for a drug identification to be confirmed to SWGDRUG specification, additional tests must includes, Infrared spectroscopy and GC-MS (Howlett and Steiner, 2011). REFERENCES: Fifield, F. W. and Kealey, D. 1995. Principles and Practice of Analytical chemistry. (4th ed) Glasgow, Blackie Academic and professional. Howlett, S. E. and Steiner, R. R. 2011. Validation of Thin Layer Chromatography with AccuTOF-DARTâ„ ¢ Detection for Forensic Drug Analysis*. Forensic Sciences [e-journal] 56 (5), pp. 1261–1267. Available through: Anglia Ruskin University Library website http://libweb.anglia.ac.uk [Accessed on 11 March 2014]. Kamberi, M., Riley, C. M., Huang, C. C. and Xiaoyan, M, 2004. A validated, sensitive HPLC method for the determination of trace impurities in acetaminophen drug substance. Pharmaceutical and Biomedical Analysis [e-journal] 34 (1), pp. 123–128. Available through: Anglia Ruskin University Library website http://libweb.anglia.ac.uk [Accessed on 18 March 2014]. Lewis, R. and Evans, W. 2011. Chemistry. 4th ed. Hampshire, Palgrave Macmillan. NCBI, 2009. National Library of Medicine. [online] Available at : http://www.ncbi.nlm.nih.gov /pccompound [Accessed 7 April, 2014]. Rubinson, J. F. and Rubinson, K. A. 1998. Contemporary chemical analysis. Upper Saddle River, NJ, Prentice Hall. Skoog, D., West, D., Holler, F. and Crouch, S. 2000. Analytical Chemistry- An introduction. (7th ed). Boca raton, Thomson Learning Inc. Tremlett, M., Anderson, B. J. and Wolf, A. 2010. Pro–con debate: is codeine a drug that still has a useful role in pediatric practice? Pediatric Anesthesia [e-journal] 20 (2), pp. 183–194. Available through: Anglia Ruskin University website http://libweb.anglia.ac.uk [Accessed on 29 March 2014].

Essay on Defining Voluntarism - 2136 Words

1. (652) In the reading of The Sources of Normativity, Christine Korsgaard discusses four basic theories for the justification of morality: Voluntarism, Realism, Reflective Endorsement, and the Appeal to Autonomy. For the purpose of this essay, I will be defining Voluntarism, outlining the argument that Korsgaard presents for Voluntarism, and explain her criticism for why it fails. First of all, let me start off by defining the meaning of Voluntarism. Voluntarism is the theory that God or the ultimate nature of reality is to be conceived as some form of will (or conation). This theory is contrasted to intellectualism, which gives primacy to God’s reason. (Internet Encyclopedia of Philosophy) The will, as referred to in the†¦show more content†¦Christine Korsgaard’s criticism for the reason why the theory of Voluntarism fails reflects upon the fact that the authority or divine power making the laws can make anything right or wrong. Korsgaard goes on to explain a si tuation in which you are a student in her department and are thereby required to take a particular course, in this case, a logic course in order to receive your degree. If you are in her department and she, having authority over you, requires you to take the course and you fail to do so, then you are at risk of not receiving your degree. On the other hand, if you are not a student in her department, she can give several reasons as to why the logic course is needed but you are not required to take the course and can hereby make a decision as to whether or not you wish to take the course, which Korsgaard goes on to explain, is why authority is needed in order to enforce the laws. You can take the course because you realize the importance, out of fear of not receiving your degree, or just for the simple fact that it is a required course. Even if the obligation was removed, the question lies among whether or not the moral agent will continue to perform the duty. It is Korsgaard’s theory that a governing body is needed to enforce the obligation in order for the action to take place and that governing body is, in what she believes, our own self. We â€Å"command ourselves† to do what is morally right, good, and just. For example, prior to theShow MoreRelatedEuthyphro, A Dialogue Written By Plato1099 Words   |  5 Pagesand the definition of theological voluntarism, it will become apparent that Euthyphro is not a theological voluntarist. This paper will first explain the definition of theological voluntarism, and what it means to be a voluntarist; next it will describe Euthyphro’s definitions of piety and the flaws of them. Finally, I will consider an objection and follow with my answer and conclusion. 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